CN113399122A - Bauxite direct flotation collecting agent and preparation method and application thereof - Google Patents
Bauxite direct flotation collecting agent and preparation method and application thereof Download PDFInfo
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- CN113399122A CN113399122A CN202110687335.5A CN202110687335A CN113399122A CN 113399122 A CN113399122 A CN 113399122A CN 202110687335 A CN202110687335 A CN 202110687335A CN 113399122 A CN113399122 A CN 113399122A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
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Abstract
The invention discloses a bauxite direct flotation collecting agent and a preparation method and application thereof. The bauxite direct flotation collecting agent is prepared from raw materials of nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether, modified monocarboxylic fatty acid and a surfactant through an emulsification reaction and a synergistic reaction; the modified monocarboxylic fatty acid has the following structure:
wherein R-represents a straight chain consisting of 14-16 carbon atoms or a hydrocarbon group containing a cyclic structure and containing one or two double bonds; r' -does not contain a carbon atom group; r' -1 to 3 carbon atoms of straight chain alkyl.The preparation method comprises the steps of emulsifier solution preparation, monocarboxylic fatty acid modification, emulsification reaction and synergistic reaction. The application is the application of the bauxite direct flotation collecting agent in preparing a collecting agent for reducing the volume of concentrate foam. The collecting agent has the characteristics of good selectivity, strong collecting capability, low medicament dosage, low temperature resistance and the like, is particularly suitable for high-iron medium-low grade bauxite, and can effectively improve the aluminum-silicon ratio of concentrate.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a bauxite direct flotation collecting agent, and a preparation method and application thereof.
Background
The bauxite resources in China are rich, the reserves are in the fourth place in the world, the types of the bauxite mainly comprise middle-low grade diasporite, which accounts for about 80%, the bauxite can be produced by the Bayer process alumina process after primary enrichment, aluminum extraction and silicon reduction, along with the development and utilization of a large amount of bauxite resources, the rich ore resources are less and less, the development and utilization of the middle-low grade bauxite are more and more urgent, and particularly, the bauxite with high iron content and middle-low grade stored in the Yunnan Shanshan area in China has great development and economic value.
The separation method of the bauxite is mainly a flotation method, the selection of the collecting agent in the mineral flotation separation process is very critical, the collecting agent enables the target mineral to float upwards along with bubbles to be a concentrate foam product by changing the hydrophilic and hydrophobic properties of the surfaces of the target mineral and the gangue mineral, and research and development of the high-efficiency collecting agent are important measures for effectively developing and utilizing the low-grade bauxite. At present, the direct flotation collector for the domestic bauxite has more defects, and is represented as follows: low temperature resistance, poor selectivity, large consumption of collecting agent, low grade of concentrate, sticky foam and difficult defoaming. Therefore, the development of an economic and efficient bauxite collecting agent is of great significance, particularly the low-grade bauxite in the high-iron of Yunnan Wenshan.
Disclosure of Invention
The first purpose of the invention is to provide a bauxite direct flotation collector; the second purpose is to provide the preparation method of the bauxite direct flotation collector; the third purpose is to provide the application of the bauxite direct flotation collector.
The first purpose of the invention is realized by that the bauxite direct flotation collecting agent is prepared by carrying out emulsification reaction and synergistic reaction on raw materials of nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether, modified monocarboxylic fatty acid and surfactant; the modified monocarboxylic fatty acid has the following structure:
wherein R-represents a straight chain consisting of 14-16 carbon atoms or a hydrocarbon group containing a cyclic structure and containing one or two double bonds;
r' -does not contain a carbon atom group;
r' -1 to 3 carbon atoms of straight chain alkyl.
The second purpose of the invention is realized by the steps of emulsifier solution preparation, monocarboxylic fatty acid modification, emulsification reaction and synergistic reaction, and specifically comprises the following steps:
A. preparing an emulsifier solution: uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a formula ratio to obtain an emulsifier solution a;
B. modification of monocarboxylic fatty acid:
1) Adding concentrated sulfuric acid into fatty acid in a constant-temperature water bath at 50-60 ℃ while stirring, and stirring at constant temperature for reaction for 0.4-0.6 h to obtain a reaction solution b;
2) adding a sodium hydroxide solution into the reaction solution b, and reacting for 1.8-2 h at the constant temperature of 90-100 ℃ to obtain modified monocarboxylic fatty acid c;
C. and (3) emulsion reaction: dropwise adding the emulsifier solution a into the modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 40-50 ℃ to obtain a mixed emulsion d;
D. and (3) synergistic reaction: and (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.5-0.8 h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector.
The specific operation method comprises the following steps:
step A: preparing an emulsifier solution: adding nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether into a reaction tank according to the mass ratio of 1:1, and uniformly stirring.
And B: modification of monocarboxylic fatty acid: (1) adding concentrated sulfuric acid into fatty acid under stirring in a constant-temperature water bath at 50-60 ℃, wherein the molar ratio of the concentrated sulfuric acid to the fatty acid is 1:1, and stirring and heating for 0.5h after the dropwise addition is finished; (2) adding a sodium hydroxide concentrated solution into the reaction solution in the step (1) according to a molar ratio of 1:1, and heating in a constant-temperature water bath at 90-100 ℃ for 1.8-2 h.
And C: and (3) emulsion reaction: and (3) placing the solution obtained in the step (B) in a constant-temperature water bath at 40-50 ℃, and dropwise adding the solution obtained in the step (A) into the solution obtained in the step (B), wherein the mass ratio of the solution obtained in the step (A) to the solution obtained in the step (B) is 0.1-0.3: 1.
Step D: and (3) synergistic reaction: and C, mixing the mixed emulsion obtained in the step C with a synergist organosilicon surfactant according to a mass ratio of 2: 0.1-0.3, and heating in a constant-temperature water bath at 40-45 ℃ for 0.5-0.8 h.
The monocarboxylic fatty acid has the following structure:
wherein R represents a straight chain or a hydrocarbon group containing a cyclic structure and consisting of 16-19 carbon atoms, and contains one or two double bonds.
The modified fatty acid has the following structure:
wherein R represents a straight-chain or cyclic hydrocarbon group having 14 to 16 carbon atoms, R 'is a group containing no carbon atom, and R' is a straight-chain hydrocarbon group having 1 to 3 carbon atoms.
The polyoxyethylene nonyl phenyl ether has the following structure:
wherein R represents a hydrocarbon group consisting of 9 carbon atoms.
The fatty alcohol-polyoxyethylene ether has the following structure:
wherein R represents a hydrocarbon group consisting of 6 to 10 carbon atoms.
The third object of the invention is realized by the application of the bauxite direct flotation collector in the preparation of a collector for reducing the volume of concentrate froth.
The bauxite direct flotation collector is prepared by modifying and compounding a fatty acid collector. After the monocarboxylic fatty acid is modified, the selectivity and the collecting capability to diaspore are improved in a targeted manner, particularly for bauxite with low aluminum-silicon ratio in high-speed iron, the aluminum-silicon ratio can be improved to more than 7.5 from about 3 by an open circuit test, and the recovery rate of open circuit aluminum is more than 85%; in addition, the dispersing performance of the agent in the ore pulp is improved through the compounding of the emulsifier and the modified fatty acid, the using amount of the collecting agent is effectively reduced, and after the surfactant is added, the effect of greatly reducing the volume of the concentrate foam is achieved, so that the subsequent flotation operation and the dewatering operation are facilitated. In a word, through modification and compounding of the monocarboxylic fatty acid, the selectivity and the collecting capacity of the collecting agent are effectively improved, the using amount is reduced, and the general problems of sticky foam and large volume of the fatty acid collecting agent are greatly improved.
Drawings
FIG. 1 is a flow chart of the process for preparing the collector for direct flotation of bauxite;
fig. 2 is a flow chart of the flotation test of the bauxite direct flotation collector.
Detailed Description
The present invention is further illustrated by the following examples and the accompanying drawings, but the present invention is not limited thereto in any way, and any modifications or alterations based on the teaching of the present invention are within the scope of the present invention.
The bauxite direct flotation collecting agent is prepared from raw materials of nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether, modified monocarboxylic fatty acid and a surfactant through an emulsification reaction and a synergistic reaction; the modified monocarboxylic fatty acid has the following structure:
wherein R-represents a straight chain consisting of 14-16 carbon atoms or a hydrocarbon group containing a cyclic structure and containing one or two double bonds;
r' -does not contain a carbon atom group;
r' -1 to 3 carbon atoms of straight chain alkyl.
The modified monocarboxylic fatty acid hydrocarbon chain contains two double bonds, and the double bonds are separated by 2-3 carbon atoms.
The mass ratio of the nonylphenol polyoxyethylene ether to the fatty alcohol polyoxyethylene ether in the nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether is 1: 1.
The polyoxyethylene nonyl phenyl ether has the following structure:
wherein R-represents a hydrocarbon group consisting of 9 carbon atoms.
The fatty alcohol-polyoxyethylene ether has the following structure:
wherein R-represents a hydrocarbon group consisting of 6 to 10 carbon atoms.
The surfactant is an organic silicon surfactant.
The preparation method of the bauxite direct flotation collecting agent comprises the steps of emulsifier solution preparation, monocarboxylic fatty acid modification, emulsification reaction and synergistic reaction, and specifically comprises the following steps:
A. preparing an emulsifier solution: uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a formula ratio to obtain an emulsifier solution a;
B. modification of monocarboxylic fatty acid:
1) adding concentrated sulfuric acid into fatty acid in a constant-temperature water bath at 50-60 ℃ while stirring, and stirring at constant temperature for reaction for 0.4-0.6 h to obtain a reaction solution b;
2) adding a sodium hydroxide solution into the reaction solution b, and reacting for 1.8-2 h at the constant temperature of 90-100 ℃ to obtain modified monocarboxylic fatty acid c;
C. and (3) emulsion reaction: dropwise adding the emulsifier solution a into the modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 40-50 ℃ to obtain a mixed emulsion d;
D. and (3) synergistic reaction: and (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.5-0.8 h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector.
The molar ratio of the concentrated sulfuric acid to the fatty acid in the step 1) is 1: 1; the molar ratio of the reaction liquid B and the sodium hydroxide solution in the step 2) in the step B is 1: 1.
The mass ratio of the emulsifier solution a to the modified monocarboxylic fatty acid c is (0.1-0.3): 1; the mass ratio of the mixed emulsion d to the surfactant is 2: (0.1-0.3).
The application of the bauxite positive flotation collecting agent is the application of the bauxite positive flotation collecting agent in the preparation of collecting agent for reducing the volume of concentrate foam.
The invention is further illustrated by the following specific examples:
example 1
Uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1 to obtain an emulsifier solution a;
adding concentrated sulfuric acid into fatty acid (the molar ratio of the concentrated sulfuric acid to the fatty acid is 1: 1) in a constant-temperature water bath at 50-55 ℃ under stirring, and stirring at constant temperature for reacting for 0.6h to obtain a reaction solution b;
adding a sodium hydroxide solution (the molar ratio of the reaction solution b to the sodium hydroxide solution is 1: 1) into the reaction solution b, and reacting for 2 hours at the constant temperature of 90-95 ℃ to obtain modified monocarboxylic fatty acid c;
dropwise adding an emulsifier solution a into modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 40-45 ℃ to obtain a mixed emulsion d, wherein the mass ratio of the emulsifier solution a to the modified monocarboxylic fatty acid c is 0.1: 1;
And (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.8h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector. Wherein the mass ratio of the mixed emulsion d to the surfactant is 2: 0.1.
Example 2
Uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1 to obtain an emulsifier solution a;
adding concentrated sulfuric acid into fatty acid (the molar ratio of the concentrated sulfuric acid to the fatty acid is 1: 1) in a constant-temperature water bath at 55-60 ℃ under stirring, and stirring at constant temperature for reacting for 0.4h to obtain a reaction solution b;
adding a sodium hydroxide solution (the molar ratio of the reaction solution b to the sodium hydroxide solution is 1: 1) into the reaction solution b, and reacting for 1.8h at the constant temperature of 95-100 ℃ to obtain modified monocarboxylic fatty acid c;
dropwise adding an emulsifier solution a into modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 45-50 ℃ to obtain a mixed emulsion d, wherein the mass ratio of the emulsifier solution a to the modified monocarboxylic fatty acid c is 0.3: 1;
and (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.5h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector. Wherein the mass ratio of the mixed emulsion d to the surfactant is 2: 0.3.
Example 3
Uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1 to obtain an emulsifier solution a;
adding concentrated sulfuric acid into fatty acid (the molar ratio of the concentrated sulfuric acid to the fatty acid is 1: 1) while stirring in a constant-temperature water bath at 53-58 ℃, and stirring at constant temperature for reacting for 0.5h to obtain a reaction solution b;
adding a sodium hydroxide solution (the molar ratio of the reaction solution b to the sodium hydroxide solution is 1: 1) into the reaction solution b, and reacting for 1.9h at the constant temperature of 93-98 ℃ to obtain modified monocarboxylic fatty acid c;
dropwise adding an emulsifier solution a into modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 43-48 ℃ to obtain a mixed emulsion d, wherein the mass ratio of the emulsifier solution a to the modified monocarboxylic fatty acid c is 0.2: 1;
and (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.7h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector. Wherein the mass ratio of the mixed emulsion d to the surfactant is 2: 0.2.
example 4
Taking bauxite in certain places of Yunnan Wenshan as an example.
The properties of raw ore: the raw material contains Al2O340.07%、SiO212.06%, Fe23.36% and the ratio of aluminum to silicon is 3.32.
The test process comprises the following steps: the roughing test flow is performed once, the grinding fineness of-0.074 mm accounts for 90%, the sodium carbonate dosage is 2000g/t, and sodium silicate is adopted: the bauxite flotation collector prepared in example 1 =2:3 combined inhibitor dosage of 600g/t and inventive collector dosage of 500 g/t. The process flow is shown in figure 2.
Mineral dressing index: aluminium concentrate Al2O349.31%，Al2O3The recovery rate is 86.26 percent, and the ratio of the concentrate to the aluminum and the silicon is 7.90.
Example 5
Taking bauxite in some places in Yunnan as an example.
The properties of raw ore: the raw material contains Al2O342.34%、SiO211.80 percent, Fe19.87 percent and the ratio of aluminum to silicon is 3.63.
The test process comprises the following steps: the roughing test flow is performed once, the grinding fineness of-0.074 mm accounts for 90%, the sodium carbonate dosage is 2000g/t, and sodium silicate is adopted: the bauxite flotation collector prepared in example 2 =3:2, the dosage of the combined inhibitor is 600g/t, and the dosage of the inventive collector is 500 g/t. The process flow is shown in figure 2.
Mineral dressing index: aluminium concentrate Al2O351.21%，Al2O3The recovery rate is 87.74%, and the ratio of aluminium to silicon in the concentrate is 7.77.
Example 6
Taking a certain bauxite in the south of Yunnan Wenshan as an example.
The properties of raw ore: the raw material contains Al2O339.23%、SiO212.21 percent, Fe22.87 percent and 3.21 percent of aluminum-silicon ratio.
The test process comprises the following steps: the roughing test flow is performed once, the grinding fineness of-0.074 mm accounts for 90%, the sodium carbonate dosage is 2000g/t, and sodium silicate is adopted: the bauxite flotation collector prepared in example 3 =1:1 combined inhibitor dosage 600g/t, and inventive collector dosage 480 g/t. The process flow is shown in figure 2.
Mineral dressing index: aluminium concentrate Al2O348.25%，Al2O3The recovery rate is 85.81%, and the ratio of aluminium to silicon in the concentrate is 7.55.
Claims (10)
1. A bauxite direct flotation collecting agent is characterized in that the bauxite direct flotation collecting agent is prepared by carrying out emulsification reaction and synergistic reaction on raw materials of nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether, modified monocarboxylic fatty acid and a surfactant; the modified monocarboxylic fatty acid has the following structure:
Wherein R-represents a straight chain consisting of 14-16 carbon atoms or a hydrocarbon group containing a cyclic structure and containing one or two double bonds;
r' -does not contain a carbon atom group;
r' -1 to 3 carbon atoms of straight chain alkyl.
2. The collector for direct flotation of bauxite according to claim 1, wherein the modified monocarboxylic fatty acid hydrocarbon chain contains two double bonds, and the double bonds are separated by 2 to 3 carbon atoms.
3. The bauxite direct flotation collector according to claim 1, wherein the mass ratio of the nonylphenol polyoxyethylene ether to the fatty alcohol polyoxyethylene ether in the nonylphenol polyoxyethylene ether-fatty alcohol polyoxyethylene ether is 1: 1.
4. The bauxite direct flotation collector according to claim 1 or 3, wherein the nonylphenol polyoxyethylene ether has the following structure:
wherein R-represents a hydrocarbon group consisting of 9 carbon atoms.
5. The bauxite direct flotation collector according to claim 1 or 3, wherein the fatty alcohol-polyoxyethylene ether has the following structure:
wherein R-represents a hydrocarbon group consisting of 6 to 10 carbon atoms.
6. The collector for direct flotation of bauxite according to claim 1, wherein the surfactant is an organosilicon surfactant.
7. A preparation method of the bauxite direct flotation collector disclosed by any one of claims 1 to 6, which is characterized by comprising the steps of emulsifier solution preparation, monocarboxylic fatty acid modification, emulsification reaction and synergistic reaction, and specifically comprises the following steps:
A. preparing an emulsifier solution: uniformly stirring nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether in a formula ratio to obtain an emulsifier solution a;
B. modification of monocarboxylic fatty acid:
1) adding concentrated sulfuric acid into fatty acid in a constant-temperature water bath at 50-60 ℃ while stirring, and stirring at constant temperature for reaction for 0.4-0.6 h to obtain a reaction solution b;
2) adding a sodium hydroxide solution into the reaction solution b, and reacting for 1.8-2 h at the constant temperature of 90-100 ℃ to obtain modified monocarboxylic fatty acid c;
C. and (3) emulsion reaction: dropwise adding the emulsifier solution a into the modified monocarboxylic fatty acid c under the condition of a constant-temperature water bath at 40-50 ℃ to obtain a mixed emulsion d;
D. and (3) synergistic reaction: and (3) mixing the mixed emulsion d with a surfactant, and then preserving the heat for 0.5-0.8 h in a constant-temperature water bath at the temperature of 40-45 ℃ to obtain the target bauxite flotation collector.
8. The method according to claim 7, wherein the molar ratio of the concentrated sulfuric acid to the fatty acid in step 1) in step B is 1: 1; the molar ratio of the reaction liquid B and the sodium hydroxide solution in the step 2) in the step B is 1: 1.
9. The method according to claim 7, wherein the mass ratio of the emulsifier solution a to the modified monocarboxylic fatty acid c is (0.1 to 0.3): 1; the mass ratio of the mixed emulsion d to the surfactant is 2: (0.1-0.3).
10. The application of the collector for the direct flotation of the bauxite according to any one of claims 1 to 6, which is characterized in that the collector for the direct flotation of the bauxite is applied to the preparation of a collector for reducing the foam volume of concentrate.
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| CN114798183A (en) | 2022-07-29 |
| CN114798183B (en) | 2024-01-23 |
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